Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email PSH@UH.EDU _publ_contact_author_name 'Prof P. Shiv Halasyamani' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University of Houston 136 Fleming Building 4800 Calhoun Blvd Houston Texas 77204-5003 UNITED STATES OF AMERICA ; _publ_section_title ; Synthesis and Characterization of Two Novel Mixed Metal Tellurates: KGaTeO5 . H2O and K3GaTe2O8(OH)2 . H2O ; loop_ _publ_author_name 'P. Shiv Halasyamani' 'Kang Min Ok' 'Ranbo Yu' data_KGaTeO5H2O _database_code_depnum_ccdc_archive 'CCDC 221436' _audit_creation_date 2003-09-09T11:36:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #---------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum 'H2 Ga1 K1 O6 Te1' _chemical_formula_weight 334.42 #---------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 10.315(5) _cell_length_b 10.438(4) _cell_length_c 10.646(5) _cell_angle_alpha 90 _cell_angle_beta 108.680(11) _cell_angle_gamma 90 _cell_volume 1085.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293.0(2) #---------------------------------------------------------------------------- _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 4.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_special_details ; ? ; #---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 11.054 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.641 #---------------------------------------------------------------------------- _diffrn_ambient_temperature 293.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method omega_scans _diffrn_reflns_av_R_equivalents 0.0913 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_number 2779 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 960 _reflns_number_gt 717 _reflns_threshold_expression >2s\(I) #---------------------------------------------------------------------------- _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #---------------------------------------------------------------------------- _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+31.2004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0002(3) _refine_ls_number_reflns 960 _refine_ls_number_parameters 63 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.012 _refine_diff_density_max 2.924 _refine_diff_density_min -2.114 _refine_diff_density_rms 0.424 #---------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.12931(11) 0.33062(11) 0.16558(11) 0.0081(4) Uani 1 1 d . . . Ga1 Ga 0.06957(18) 0.10349(18) 0.34355(18) 0.0097(5) Uani 1 1 d . . . K1 K 0.2492(19) -0.1979(10) 0.4625(13) 0.071(4) Uani 0.607(11) 1 d P . . K2 K 0.0562(19) -0.0560(19) 0.061(2) 0.071(4) Uani 0.360(11) 1 d P . . O1 O 0.2549(12) 0.1958(11) 0.1475(11) 0.011(3) Uiso 1 1 d . . . O2 O 0.0075(11) 0.2061(11) 0.1920(11) 0.008(2) Uiso 1 1 d . . . O3 O 0.2466(12) 0.0473(12) 0.3627(11) 0.013(3) Uiso 1 1 d . . . O4 O 0.0260(12) 0.1718(12) 0.4841(12) 0.016(3) Uiso 1 1 d . . . O5 O -0.0319(12) -0.0414(12) 0.2819(12) 0.017(3) Uiso 1 1 d . . . OW1 O 0.090(2) 0.029(2) -0.021(2) 0.035(5) Uiso 0.71(3) 1 d P . . OW2 O 0.183(5) -0.032(5) 0.000(5) 0.035(5) Uiso 0.29(2) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0055(6) 0.0110(6) 0.0082(6) 0.0024(5) 0.0025(4) 0.0014(5) Ga1 0.0081(10) 0.0107(11) 0.0109(10) 0.0008(8) 0.0037(8) -0.0002(8) K1 0.045(5) 0.051(6) 0.102(12) 0.012(5) 0.005(8) -0.014(5) K2 0.045(5) 0.051(6) 0.102(12) 0.012(5) 0.005(8) -0.014(5) #---------------------------------------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 O5 1.862(12) 4_455 ? Te1 O4 1.885(12) 8_554 ? Te1 O2 1.890(11) . ? Te1 O3 1.897(12) 7 ? Te1 O1 1.964(11) . ? Te1 O1 1.985(12) 7 ? Te1 Te1 3.065(2) 7 ? Te1 K1 3.712(19) 4_455 ? Te1 K2 3.84(2) 5 ? Te1 K1 3.835(18) 3_454 ? Ga1 O5 1.837(13) . ? Ga1 O4 1.838(12) . ? Ga1 O3 1.866(12) . ? Ga1 O2 1.871(11) . ? Ga1 K2 3.40(2) . ? Ga1 K1 3.665(14) . ? Ga1 K1 3.897(12) 2_556 ? Ga1 K1 4.022(17) 6 ? K1 K1 0.79(3) 2_556 ? K1 O3 2.769(16) . ? K1 O2 2.82(2) 4_445 ? K1 O4 2.80(2) 6_655 ? K1 OW2 2.90(6) 7_545 ? K1 OW2 2.95(6) 8_545 ? K1 O4 3.08(2) 5_556 ? K1 O2 3.147(19) 3_545 ? K1 O3 3.157(17) 2_556 ? K1 K2 3.32(3) 7_545 ? K1 O5 3.35(2) . ? K1 K2 3.61(3) 8_545 ? K2 OW1 1.36(3) . ? K2 OW1 1.45(3) 5 ? K2 OW2 1.66(6) . ? K2 K2 1.85(4) 5 ? K2 OW2 2.52(6) 5 ? K2 O5 2.78(3) . ? K2 OW2 2.97(6) 2 ? K2 O4 2.96(2) 4_445 ? K2 O2 3.00(3) 5 ? K2 O2 3.18(3) . ? K2 O1 3.28(2) . ? K2 K1 3.32(3) 7_545 ? O1 Te1 1.985(12) 7 ? O2 K1 2.82(2) 4_455 ? O2 K2 3.00(3) 5 ? O2 K1 3.147(19) 3_454 ? O3 Te1 1.897(12) 7 ? O3 K1 3.157(17) 2_556 ? O4 Te1 1.885(12) 8 ? O4 K1 2.80(2) 6 ? O4 K2 2.96(2) 4_455 ? O4 K1 3.08(2) 5_556 ? O5 Te1 1.862(12) 4_445 ? OW1 OW2 1.12(5) . ? OW1 K2 1.45(3) 5 ? OW2 OW2 1.38(10) 2 ? OW2 K2 2.52(6) 5 ? OW2 K2 2.97(6) 2 ? OW2 K1 2.90(6) 7_545 ? OW2 K1 2.95(6) 8_544 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Te1 O4 97.8(5) 4_455 8_554 ? O5 Te1 O2 90.0(5) 4_455 . ? O4 Te1 O2 87.6(5) 8_554 . ? O5 Te1 O3 91.3(5) 4_455 7 ? O4 Te1 O3 92.0(5) 8_554 7 ? O2 Te1 O3 178.7(5) . 7 ? O5 Te1 O1 168.6(5) 4_455 . ? O4 Te1 O1 93.7(5) 8_554 . ? O2 Te1 O1 90.7(5) . . ? O3 Te1 O1 88.0(5) 7 . ? O5 Te1 O1 90.4(5) 4_455 7 ? O4 Te1 O1 170.8(5) 8_554 7 ? O2 Te1 O1 88.3(5) . 7 ? O3 Te1 O1 91.9(5) 7 7 ? O1 Te1 O1 78.2(5) . 7 ? O5 Te1 Te1 129.3(4) 4_455 7 ? O4 Te1 Te1 132.9(4) 8_554 7 ? O2 Te1 Te1 89.4(3) . 7 ? O3 Te1 Te1 90.0(4) 7 7 ? O1 Te1 Te1 39.3(3) . 7 ? O1 Te1 Te1 38.8(3) 7 7 ? O5 Te1 K1 64.1(4) 4_455 4_455 ? O4 Te1 K1 55.9(4) 8_554 4_455 ? O2 Te1 K1 47.8(4) . 4_455 ? O3 Te1 K1 132.8(4) 7 4_455 ? O1 Te1 K1 123.8(4) . 4_455 ? O1 Te1 K1 125.5(4) 7 4_455 ? Te1 Te1 K1 137.09(19) 7 4_455 ? O5 Te1 K2 121.1(5) 4_455 5 ? O4 Te1 K2 48.8(5) 8_554 5 ? O2 Te1 K2 50.1(5) . 5 ? O3 Te1 K2 128.9(5) 7 5 ? O1 Te1 K2 67.4(4) . 5 ? O1 Te1 K2 123.0(4) 7 5 ? Te1 Te1 K2 96.1(3) 7 5 ? K1 Te1 K2 57.0(3) 4_455 5 ? O5 Te1 K1 70.9(4) 4_455 3_454 ? O4 Te1 K1 44.0(4) 8_554 3_454 ? O2 Te1 K1 54.7(4) . 3_454 ? O3 Te1 K1 125.6(4) 7 3_454 ? O1 Te1 K1 118.5(4) . 3_454 ? O1 Te1 K1 137.1(4) 7 3_454 ? Te1 Te1 K1 141.23(17) 7 3_454 ? K1 Te1 K1 11.9(4) 4_455 3_454 ? K2 Te1 K1 51.2(3) 5 3_454 ? O5 Ga1 O4 110.5(5) . . ? O5 Ga1 O3 101.9(5) . . ? O4 Ga1 O3 121.2(5) . . ? O5 Ga1 O2 99.5(5) . . ? O4 Ga1 O2 112.0(5) . . ? O3 Ga1 O2 109.1(5) . . ? O5 Ga1 K2 54.8(5) . . ? O4 Ga1 K2 163.4(5) . . ? O3 Ga1 K2 72.8(5) . . ? O2 Ga1 K2 67.1(5) . . ? O5 Ga1 K1 65.4(5) . . ? O4 Ga1 K1 106.3(5) . . ? O3 Ga1 K1 47.4(5) . . ? O2 Ga1 K1 141.7(4) . . ? K2 Ga1 K1 76.0(4) . . ? O5 Ga1 K1 69.3(5) . 2_556 ? O4 Ga1 K1 94.7(4) . 2_556 ? O3 Ga1 K1 53.3(5) . 2_556 ? O2 Ga1 K1 153.2(4) . 2_556 ? K2 Ga1 K1 87.1(4) . 2_556 ? K1 Ga1 K1 11.5(4) . 2_556 ? O5 Ga1 K1 83.3(4) . 6 ? O4 Ga1 K1 37.7(4) . 6 ? O3 Ga1 K1 156.4(4) . 6 ? O2 Ga1 K1 92.4(4) . 6 ? K2 Ga1 K1 126.4(4) . 6 ? K1 Ga1 K1 118.5(4) . 6 ? K1 Ga1 K1 109.5(3) 2_556 6 ? K1 K1 O3 112.4(4) 2_556 . ? K1 K1 O2 107(3) 2_556 4_445 ? O3 K1 O2 102.3(6) . 4_445 ? K1 K1 O4 103(3) 2_556 6_655 ? O3 K1 O4 80.0(5) . 6_655 ? O2 K1 O4 145.6(6) 4_445 6_655 ? K1 K1 OW2 86.2(13) 2_556 7_545 ? O3 K1 OW2 157.6(12) . 7_545 ? O2 K1 OW2 82.8(11) 4_445 7_545 ? O4 K1 OW2 83.7(11) 6_655 7_545 ? K1 K1 OW2 78.3(13) 2_556 8_545 ? O3 K1 OW2 163.5(12) . 8_545 ? O2 K1 OW2 61.6(11) 4_445 8_545 ? O4 K1 OW2 110.8(12) 6_655 8_545 ? OW2 K1 OW2 27(2) 7_545 8_545 ? K1 K1 O4 62(3) 2_556 5_556 ? O3 K1 O4 95.3(6) . 5_556 ? O2 K1 O4 52.4(4) 4_445 5_556 ? O4 K1 O4 161.9(6) 6_655 5_556 ? OW2 K1 O4 104.8(11) 7_545 5_556 ? OW2 K1 O4 78.1(11) 8_545 5_556 ? K1 K1 O2 59(2) 2_556 3_545 ? O3 K1 O2 119.6(6) . 3_545 ? O2 K1 O2 138.1(6) 4_445 3_545 ? O4 K1 O2 51.7(4) 6_655 3_545 ? OW2 K1 O2 58.4(11) 7_545 3_545 ? OW2 K1 O2 76.5(11) 8_545 3_545 ? O4 K1 O2 119.1(5) 5_556 3_545 ? K1 K1 O3 54.2(3) 2_556 2_556 ? O3 K1 O3 58.2(5) . 2_556 ? O2 K1 O3 117.7(7) 4_445 2_556 ? O4 K1 O3 92.9(5) 6_655 2_556 ? OW2 K1 O3 138.5(12) 7_545 2_556 ? OW2 K1 O3 130.9(12) 8_545 2_556 ? O4 K1 O3 70.0(5) 5_556 2_556 ? O2 K1 O3 87.3(5) 3_545 2_556 ? K1 K1 K2 104.9(17) 2_556 7_545 ? O3 K1 K2 128.2(7) . 7_545 ? O2 K1 K2 99.2(5) 4_445 7_545 ? O4 K1 K2 57.1(5) 6_655 7_545 ? OW2 K1 K2 30.0(11) 7_545 7_545 ? OW2 K1 K2 56.2(11) 8_545 7_545 ? O4 K1 K2 134.2(5) 5_556 7_545 ? O2 K1 K2 55.2(5) 3_545 7_545 ? O3 K1 K2 141.1(7) 2_556 7_545 ? K1 K1 O5 108(2) 2_556 . ? O3 K1 O5 55.1(4) . . ? O2 K1 O5 50.1(4) 4_445 . ? O4 K1 O5 132.2(5) 6_655 . ? OW2 K1 O5 132.9(12) 7_545 . ? OW2 K1 O5 110.3(12) 8_545 . ? O4 K1 O5 51.9(4) 5_556 . ? O2 K1 O5 164.5(5) 3_545 . ? O3 K1 O5 77.8(4) 2_556 . ? K2 K1 O5 140.2(6) 7_545 . ? K1 K1 K2 62.8(16) 2_556 8_545 ? O3 K1 K2 146.3(8) . 8_545 ? O2 K1 K2 54.0(5) 4_445 8_545 ? O4 K1 K2 133.5(6) 6_655 8_545 ? OW2 K1 K2 53.0(11) 7_545 8_545 ? OW2 K1 K2 27.0(11) 8_545 8_545 ? O4 K1 K2 51.8(5) 5_556 8_545 ? O2 K1 K2 87.5(5) 3_545 8_545 ? O3 K1 K2 108.1(6) 2_556 8_545 ? K2 K1 K2 82.8(7) 7_545 8_545 ? O5 K1 K2 93.3(6) . 8_545 ? OW1 K2 OW1 97.9(18) . 5 ? OW1 K2 OW2 42(2) . . ? OW1 K2 OW2 137(3) 5 . ? OW1 K2 K2 51.1(14) . 5 ? OW1 K2 K2 46.8(12) 5 5 ? OW2 K2 K2 92(2) . 5 ? OW1 K2 OW2 91.5(18) . 5 ? OW1 K2 OW2 10.4(16) 5 5 ? OW2 K2 OW2 132.7(18) . 5 ? K2 K2 OW2 41.2(15) 5 5 ? OW1 K2 O5 136.3(16) . . ? OW1 K2 O5 69.5(13) 5 . ? OW2 K2 O5 147(2) . . ? K2 K2 O5 104.9(16) 5 . ? OW2 K2 O5 68.8(14) 5 . ? OW1 K2 OW2 51.3(16) . 2 ? OW1 K2 OW2 147.6(18) 5 2 ? OW2 K2 OW2 11(3) . 2 ? K2 K2 OW2 101.7(18) 5 2 ? OW2 K2 OW2 142.7(17) 5 2 ? O5 K2 OW2 137.9(13) . 2 ? OW1 K2 O4 129.7(16) . 4_445 ? OW1 K2 O4 85.5(12) 5 4_445 ? OW2 K2 O4 107(2) . 4_445 ? K2 K2 O4 114.1(14) 5 4_445 ? OW2 K2 O4 96.0(14) 5 4_445 ? O5 K2 O4 92.0(7) . 4_445 ? OW2 K2 O4 106.1(13) 2 4_445 ? OW1 K2 O2 78.1(14) . 5 ? OW1 K2 O2 85.9(13) 5 5 ? OW2 K2 O2 72(2) . 5 ? K2 K2 O2 78.0(14) 5 5 ? OW2 K2 O2 92.7(14) 5 5 ? O5 K2 O2 138.5(7) . 5 ? OW2 K2 O2 78.6(12) 2 5 ? O4 K2 O2 52.0(5) 4_445 5 ? OW1 K2 O2 80.2(13) . . ? OW1 K2 O2 70.6(13) 5 . ? OW2 K2 O2 108(2) . . ? K2 K2 O2 67.3(13) 5 . ? OW2 K2 O2 61.2(13) 5 . ? O5 K2 O2 56.1(6) . . ? OW2 K2 O2 107.8(12) 2 . ? O4 K2 O2 145.0(8) 4_445 . ? O2 K2 O2 145.3(7) 5 . ? OW1 K2 O1 52.7(11) . . ? OW1 K2 O1 115.0(14) 5 . ? OW2 K2 O1 59(2) . . ? K2 K2 O1 83.5(12) 5 . ? OW2 K2 O1 104.6(14) 5 . ? O5 K2 O1 93.6(7) . . ? OW2 K2 O1 57.8(11) 2 . ? O4 K2 O1 159.4(8) 4_445 . ? O2 K2 O1 127.5(8) 5 . ? O2 K2 O1 50.2(4) . . ? OW1 K2 K1 99.9(15) . 7_545 ? OW1 K2 K1 136.2(14) 5 7_545 ? OW2 K2 K1 61(2) . 7_545 ? K2 K2 K1 133.9(18) 5 7_545 ? OW2 K2 K1 146.2(14) 5 7_545 ? O5 K2 K1 118.4(7) . 7_545 ? OW2 K2 K1 55.7(12) 2 7_545 ? O4 K2 K1 52.7(5) 4_445 7_545 ? O2 K2 K1 59.5(5) 5 7_545 ? O2 K2 K1 152.0(7) . 7_545 ? O1 K2 K1 107.6(6) . 7_545 ? Te1 O1 Te1 101.8(5) . 7 ? Te1 O1 K2 103.3(6) . . ? Te1 O1 K2 106.9(6) 7 . ? Ga1 O2 Te1 117.5(6) . . ? Ga1 O2 K1 134.8(6) . 4_455 ? Te1 O2 K1 102.4(5) . 4_455 ? Ga1 O2 K2 113.0(6) . 5 ? Te1 O2 K2 101.0(6) . 5 ? K1 O2 K2 76.5(5) 4_455 5 ? Ga1 O2 K1 145.4(6) . 3_454 ? Te1 O2 K1 95.9(5) . 3_454 ? K1 O2 K1 13.9(6) 4_455 3_454 ? K2 O2 K1 65.3(5) 5 3_454 ? Ga1 O2 K2 80.1(5) . . ? Te1 O2 K2 108.7(6) . . ? K1 O2 K2 107.5(6) 4_455 . ? K2 O2 K2 34.7(7) 5 . ? K1 O2 K2 98.4(5) 3_454 . ? Ga1 O3 Te1 117.3(6) . 7 ? Ga1 O3 K1 102.8(6) . . ? Te1 O3 K1 139.3(7) 7 . ? Ga1 O3 K1 98.5(6) . 2_556 ? Te1 O3 K1 139.1(6) 7 2_556 ? K1 O3 K1 13.5(5) . 2_556 ? Ga1 O3 K2 75.2(5) . . ? Te1 O3 K2 106.3(6) 7 . ? K1 O3 K2 90.0(6) . . ? K1 O3 K2 101.3(5) 2_556 . ? Ga1 O4 Te1 128.6(7) . 8 ? Ga1 O4 K1 118.6(6) . 6 ? Te1 O4 K1 108.2(6) 8 6 ? Ga1 O4 K2 111.9(7) . 4_455 ? Te1 O4 K2 102.6(6) 8 4_455 ? K1 O4 K2 70.2(5) 6 4_455 ? Ga1 O4 K1 131.7(6) . 5_556 ? Te1 O4 K1 93.7(5) 8 5_556 ? K1 O4 K1 14.5(5) 6 5_556 ? K2 O4 K1 73.3(5) 4_455 5_556 ? Ga1 O5 Te1 141.6(7) . 4_445 ? Ga1 O5 K2 92.5(6) . . ? Te1 O5 K2 124.6(7) 4_445 . ? Ga1 O5 K1 84.7(5) . . ? Te1 O5 K1 85.9(5) 4_445 . ? K2 O5 K1 90.1(6) . . ? OW2 OW1 K2 83(3) . . ? OW2 OW1 K2 156(4) . 5 ? K2 OW1 K2 82.1(18) . 5 ? OW1 OW2 OW2 143(4) . 2 ? OW1 OW2 K2 55(3) . . ? OW2 OW2 K2 156(6) 2 . ? OW1 OW2 K2 14(2) . 5 ? OW2 OW2 K2 154(3) 2 5 ? K2 OW2 K2 47.3(18) . 5 ? OW1 OW2 K2 142(4) . 2 ? OW2 OW2 K2 13(3) 2 2 ? K2 OW2 K2 163(3) . 2 ? K2 OW2 K2 149(2) 5 2 ? OW1 OW2 K1 138(4) . 7_545 ? OW2 OW2 K1 78.6(12) 2 7_545 ? K2 OW2 K1 89(2) . 7_545 ? K2 OW2 K1 124(2) 5 7_545 ? K2 OW2 K1 75.9(14) 2 7_545 ? OW1 OW2 K1 138(4) . 8_544 ? OW2 OW2 K1 74.2(12) 2 8_544 ? K2 OW2 K1 99(2) . 8_544 ? K2 OW2 K1 124(2) 5 8_544 ? K2 OW2 K1 68.2(13) 2 8_544 ? K1 OW2 K1 15.6(6) 7_545 8_544 ? #===End data_K3GaTe2O8(OH)2H2O _database_code_depnum_ccdc_archive 'CCDC 221437' _audit_creation_date 2003-09-09T11:40:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #---------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum 'H4 Ga K3 O11 Te2' _chemical_formula_weight 622.22 #---------------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4369(9) _cell_length_b 7.4903(9) _cell_length_c 11.4128(15) _cell_angle_alpha 84.071(2) _cell_angle_beta 75.065(2) _cell_angle_gamma 62.227(2) _cell_volume 543.40(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293.0(2) #---------------------------------------------------------------------------- _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 3.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_special_details ; ? ; #---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 8.991 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.557 #---------------------------------------------------------------------------- _diffrn_ambient_temperature 293.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemen Smart' _diffrn_measurement_method omega_scan _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_number 3327 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.98 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.891 _diffrn_measured_fraction_theta_max 0.891 _reflns_number_total 2331 _reflns_number_gt 2066 _reflns_threshold_expression >2s\(I) #---------------------------------------------------------------------------- _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #---------------------------------------------------------------------------- _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+21.4505P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0051(6) _refine_ls_number_reflns 2331 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.153 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.319 #---------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.12959(11) 0.11396(10) 0.45348(6) 0.0101(2) Uani 1 1 d . . . Te2 Te 0.20777(11) -0.19967(10) -0.02800(6) 0.0116(2) Uani 1 1 d . . . Ga1 Ga 0.99073(18) -0.05170(18) 0.25366(10) 0.0107(3) Uani 1 1 d . . . K1 K 0.5534(4) -0.1132(4) 0.1647(2) 0.0220(6) Uani 1 1 d . . . K2 K 0.0706(4) 0.4100(4) 0.1629(2) 0.0217(6) Uani 1 1 d . . . K3 K 0.5639(6) 0.5764(6) 0.6470(4) 0.0477(10) Uani 1 1 d . . . O1 O 0.1661(12) -0.1604(11) 0.5034(7) 0.0121(15) Uani 1 1 d . . . O2 O 0.4211(12) 0.0272(13) 0.4102(7) 0.0167(17) Uani 1 1 d . . . O3 O 0.8994(13) -0.1785(12) 0.3820(7) 0.0161(16) Uani 1 1 d . . . O4 O 1.1470(12) 0.0579(12) 0.2895(7) 0.0138(15) Uani 1 1 d . . . O5 O 0.0552(13) 0.3856(11) 0.4117(7) 0.0165(16) Uani 1 1 d . . . O6 O -0.0986(13) -0.0925(12) -0.0149(7) 0.0158(16) Uani 1 1 d . . . O7 O 0.7630(12) 0.1297(12) 0.1958(6) 0.0131(15) Uani 1 1 d . . . O8 O 0.4838(12) -0.2449(12) -0.0411(8) 0.0173(17) Uani 1 1 d . . . O9 O 1.1679(12) -0.2594(11) 0.1413(7) 0.0139(15) Uani 1 1 d . . . O10 O 0.2633(13) -0.4644(12) -0.0644(8) 0.0179(17) Uani 1 1 d . . . OW1 O 0.3398(15) 0.3874(14) 0.6370(10) 0.032(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0121(4) 0.0129(4) 0.0080(3) 0.0005(2) -0.0025(2) -0.0080(3) Te2 0.0108(4) 0.0115(4) 0.0086(3) -0.0005(2) -0.0016(2) -0.0021(3) Ga1 0.0127(6) 0.0122(6) 0.0086(5) 0.0008(4) -0.0035(4) -0.0064(5) K1 0.0229(13) 0.0222(13) 0.0209(13) -0.0004(10) -0.0024(10) -0.0116(11) K2 0.0287(14) 0.0224(13) 0.0178(12) 0.0045(10) -0.0071(10) -0.0149(12) K3 0.0383(19) 0.054(2) 0.057(2) -0.0267(18) 0.0154(16) -0.0345(18) O1 0.012(4) 0.014(4) 0.013(4) 0.005(3) -0.005(3) -0.008(3) O2 0.012(4) 0.030(5) 0.010(4) 0.003(3) -0.003(3) -0.011(4) O3 0.025(4) 0.020(4) 0.007(3) 0.000(3) -0.004(3) -0.014(4) O4 0.018(4) 0.020(4) 0.008(3) 0.000(3) -0.004(3) -0.012(3) O5 0.022(4) 0.010(4) 0.019(4) -0.003(3) -0.003(3) -0.008(3) O6 0.018(4) 0.012(4) 0.018(4) 0.001(3) -0.009(3) -0.006(3) O7 0.013(4) 0.017(4) 0.006(3) -0.002(3) -0.003(3) -0.003(3) O8 0.010(4) 0.020(4) 0.025(4) 0.002(3) -0.005(3) -0.009(3) O9 0.015(4) 0.011(4) 0.013(4) 0.004(3) -0.004(3) -0.003(3) O10 0.019(4) 0.014(4) 0.027(4) -0.005(3) -0.009(3) -0.011(3) OW1 0.030(5) 0.023(5) 0.044(6) -0.005(4) -0.011(4) -0.010(4) #---------------------------------------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 O5 1.887(8) . ? Te1 O2 1.889(8) . ? Te1 O4 1.919(7) 1_455 ? Te1 O3 1.920(7) 2_656 ? Te1 O1 1.985(7) . ? Te1 O1 1.991(7) 2_556 ? Te1 Te1 3.0651(13) 2_556 ? Te1 K2 3.799(3) . ? Te1 K1 3.807(3) . ? Te1 K3 3.863(3) 2_666 ? Te2 O8 1.885(8) . ? Te2 O10 1.896(8) . ? Te2 O9 1.916(8) 1_455 ? Te2 O7 1.917(7) 2_655 ? Te2 O6 2.001(8) . ? Te2 O6 2.012(8) 2 ? Te2 Te2 3.1093(14) 2 ? Te2 K1 3.574(3) 2_655 ? Te2 K2 3.784(3) 2 ? Te2 K2 3.828(3) 1_545 ? Te2 K3 3.958(4) 1_544 ? Te2 K1 4.077(3) . ? Ga1 O3 1.819(8) . ? Ga1 O4 1.842(8) . ? Ga1 O7 1.843(8) . ? Ga1 O9 1.852(8) . ? Ga1 K2 3.774(3) 1_655 ? Ga1 K1 3.855(3) 1_655 ? Ga1 K1 3.875(3) . ? Ga1 K3 3.964(4) 2_666 ? Ga1 K2 4.000(3) 1_645 ? K1 O4 2.712(8) 1_455 ? K1 O8 2.827(9) 2_655 ? K1 O2 2.854(8) . ? K1 O8 2.889(9) . ? K1 OW1 2.901(11) 2_656 ? K1 O6 2.915(9) 1_655 ? K1 O7 2.987(8) . ? K1 O10 3.017(8) 2_645 ? K1 Te2 3.574(3) 2_655 ? K1 K2 3.837(4) 1_645 ? K1 Ga1 3.855(3) 1_455 ? K2 O4 2.758(8) 1_455 ? K2 O5 2.803(8) . ? K2 O10 2.828(8) 2 ? K2 O9 2.858(8) 1_465 ? K2 O10 2.916(9) 1_565 ? K2 O8 2.934(8) 2_655 ? K2 O6 2.955(8) 2 ? K2 OW1 3.105(11) 2_566 ? K2 Ga1 3.774(3) 1_455 ? K2 Te2 3.784(3) 2 ? K2 Te2 3.828(3) 1_565 ? K3 OW1 2.669(10) . ? K3 O7 2.749(8) 2_666 ? K3 O5 2.879(9) 2_666 ? K3 O2 3.020(9) 2_666 ? K3 OW1 3.146(11) 2_666 ? K3 O1 3.192(8) 2_656 ? K3 O1 3.423(9) 1_565 ? K3 Te1 3.863(3) 2_666 ? K3 K2 3.931(5) 2_666 ? K3 Te2 3.958(4) 1_566 ? K3 Ga1 3.964(4) 2_666 ? K3 K3 4.114(8) 2_666 ? O1 Te1 1.991(7) 2_556 ? O1 K3 3.192(8) 2_656 ? O1 K3 3.423(9) 1_545 ? O2 K3 3.020(9) 2_666 ? O3 Te1 1.920(7) 2_656 ? O4 Te1 1.919(7) 1_655 ? O4 K1 2.712(8) 1_655 ? O4 K2 2.758(8) 1_655 ? O5 K3 2.879(9) 2_666 ? O6 Te2 2.012(8) 2 ? O6 K1 2.915(9) 1_455 ? O6 K2 2.955(8) 2 ? O7 Te2 1.917(7) 2_655 ? O7 K3 2.749(8) 2_666 ? O8 K1 2.827(9) 2_655 ? O8 K2 2.934(8) 2_655 ? O9 Te2 1.916(8) 1_655 ? O9 K2 2.858(8) 1_645 ? O10 K2 2.828(8) 2 ? O10 K2 2.916(9) 1_545 ? O10 K1 3.017(8) 2_645 ? OW1 K1 2.901(11) 2_656 ? OW1 K2 3.105(11) 2_566 ? OW1 K3 3.146(11) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Te1 O2 95.3(4) . . ? O5 Te1 O4 88.8(3) . 1_455 ? O2 Te1 O4 88.4(3) . 1_455 ? O5 Te1 O3 89.9(3) . 2_656 ? O2 Te1 O3 93.6(3) . 2_656 ? O4 Te1 O3 177.7(4) 1_455 2_656 ? O5 Te1 O1 172.1(3) . . ? O2 Te1 O1 92.5(3) . . ? O4 Te1 O1 91.3(3) 1_455 . ? O3 Te1 O1 89.8(3) 2_656 . ? O5 Te1 O1 93.0(3) . 2_556 ? O2 Te1 O1 171.1(3) . 2_556 ? O4 Te1 O1 88.7(3) 1_455 2_556 ? O3 Te1 O1 89.5(3) 2_656 2_556 ? O1 Te1 O1 79.1(3) . 2_556 ? O5 Te1 Te1 132.5(3) . 2_556 ? O2 Te1 Te1 132.1(3) . 2_556 ? O4 Te1 Te1 90.0(2) 1_455 2_556 ? O3 Te1 Te1 89.5(2) 2_656 2_556 ? O1 Te1 Te1 39.6(2) . 2_556 ? O1 Te1 Te1 39.5(2) 2_556 2_556 ? O5 Te1 K2 45.0(2) . . ? O2 Te1 K2 90.5(2) . . ? O4 Te1 K2 43.9(2) 1_455 . ? O3 Te1 K2 134.9(2) 2_656 . ? O1 Te1 K2 134.9(2) . . ? O1 Te1 K2 93.2(2) 2_556 . ? Te1 Te1 K2 119.58(5) 2_556 . ? O5 Te1 K1 95.9(2) . . ? O2 Te1 K1 46.4(2) . . ? O4 Te1 K1 42.2(2) 1_455 . ? O3 Te1 K1 139.9(3) 2_656 . ? O1 Te1 K1 89.5(2) . . ? O1 Te1 K1 129.6(2) 2_556 . ? Te1 Te1 K1 114.04(5) 2_556 . ? K2 Te1 K1 61.57(6) . . ? O5 Te1 K3 45.6(3) . 2_666 ? O2 Te1 K3 50.1(3) . 2_666 ? O4 Te1 K3 92.9(2) 1_455 2_666 ? O3 Te1 K3 87.6(2) 2_656 2_666 ? O1 Te1 K3 142.2(2) . 2_666 ? O1 Te1 K3 138.5(2) 2_556 2_666 ? Te1 Te1 K3 176.50(6) 2_556 2_666 ? K2 Te1 K3 61.73(8) . 2_666 ? K1 Te1 K3 69.45(7) . 2_666 ? O8 Te2 O10 99.2(3) . . ? O8 Te2 O9 92.5(3) . 1_455 ? O10 Te2 O9 89.8(3) . 1_455 ? O8 Te2 O7 89.0(3) . 2_655 ? O10 Te2 O7 91.8(3) . 2_655 ? O9 Te2 O7 177.6(3) 1_455 2_655 ? O8 Te2 O6 168.4(3) . . ? O10 Te2 O6 92.1(3) . . ? O9 Te2 O6 90.4(3) 1_455 . ? O7 Te2 O6 87.8(3) 2_655 . ? O8 Te2 O6 90.3(3) . 2 ? O10 Te2 O6 170.5(3) . 2 ? O9 Te2 O6 89.3(3) 1_455 2 ? O7 Te2 O6 88.8(3) 2_655 2 ? O6 Te2 O6 78.4(3) . 2 ? O8 Te2 Te2 129.3(3) . 2 ? O10 Te2 Te2 131.5(2) . 2 ? O9 Te2 Te2 89.8(2) 1_455 2 ? O7 Te2 Te2 87.8(2) 2_655 2 ? O6 Te2 Te2 39.3(2) . 2 ? O6 Te2 Te2 39.1(2) 2 2 ? O8 Te2 K1 51.8(3) . 2_655 ? O10 Te2 K1 132.7(3) . 2_655 ? O9 Te2 K1 123.1(2) 1_455 2_655 ? O7 Te2 K1 56.7(2) 2_655 2_655 ? O6 Te2 K1 117.8(2) . 2_655 ? O6 Te2 K1 54.6(2) 2 2_655 ? Te2 Te2 K1 85.70(5) 2 2_655 ? O8 Te2 K2 138.2(3) . 2 ? O10 Te2 K2 46.3(2) . 2 ? O9 Te2 K2 107.3(2) 1_455 2 ? O7 Te2 K2 72.6(2) 2_655 2 ? O6 Te2 K2 50.7(2) . 2 ? O6 Te2 K2 125.3(2) 2 2 ? Te2 Te2 K2 88.10(5) 2 2 ? K1 Te2 K2 129.05(6) 2_655 2 ? O8 Te2 K2 113.7(3) . 1_545 ? O10 Te2 K2 47.8(3) . 1_545 ? O9 Te2 K2 46.2(2) 1_455 1_545 ? O7 Te2 K2 134.6(2) 2_655 1_545 ? O6 Te2 K2 76.1(2) . 1_545 ? O6 Te2 K2 127.4(2) 2 1_545 ? Te2 Te2 K2 103.78(5) 2 1_545 ? K1 Te2 K2 164.59(6) 2_655 1_545 ? K2 Te2 K2 64.28(7) 2 1_545 ? O8 Te2 K3 69.4(3) . 1_544 ? O10 Te2 K3 63.5(3) . 1_544 ? O9 Te2 K3 143.3(2) 1_455 1_544 ? O7 Te2 K3 39.0(2) 2_655 1_544 ? O6 Te2 K3 114.0(2) . 1_544 ? O6 Te2 K3 121.1(2) 2 1_544 ? Te2 Te2 K3 126.57(8) 2 1_544 ? K1 Te2 K3 70.71(7) 2_655 1_544 ? K2 Te2 K3 73.15(7) 2 1_544 ? K2 Te2 K3 111.22(7) 1_545 1_544 ? O8 Te2 K1 39.7(3) . . ? O10 Te2 K1 120.3(2) . . ? O9 Te2 K1 61.6(2) 1_455 . ? O7 Te2 K1 118.9(2) 2_655 . ? O6 Te2 K1 134.7(2) . . ? O6 Te2 K1 67.2(2) 2 . ? Te2 Te2 K1 101.63(5) 2 . ? K1 Te2 K1 63.97(7) 2_655 . ? K2 Te2 K1 164.85(6) 2 . ? K2 Te2 K1 101.79(6) 1_545 . ? K3 Te2 K1 108.92(7) 1_544 . ? O3 Ga1 O4 112.7(3) . . ? O3 Ga1 O7 108.1(4) . . ? O4 Ga1 O7 114.5(4) . . ? O3 Ga1 O9 103.3(3) . . ? O4 Ga1 O9 107.5(3) . . ? O7 Ga1 O9 110.1(3) . . ? O3 Ga1 K2 143.7(2) . 1_655 ? O4 Ga1 K2 43.8(2) . 1_655 ? O7 Ga1 K2 73.4(3) . 1_655 ? O9 Ga1 K2 110.2(2) . 1_655 ? O3 Ga1 K1 122.9(3) . 1_655 ? O4 Ga1 K1 39.9(2) . 1_655 ? O7 Ga1 K1 128.4(3) . 1_655 ? O9 Ga1 K1 67.7(3) . 1_655 ? K2 Ga1 K1 61.36(6) 1_655 1_655 ? O3 Ga1 K1 75.8(3) . . ? O4 Ga1 K1 162.7(3) . . ? O7 Ga1 K1 48.4(3) . . ? O9 Ga1 K1 83.9(3) . . ? K2 Ga1 K1 120.59(7) 1_655 . ? K1 Ga1 K1 148.33(8) 1_655 . ? O3 Ga1 K3 86.4(3) . 2_666 ? O4 Ga1 K3 97.1(3) . 2_666 ? O7 Ga1 K3 37.8(2) . 2_666 ? O9 Ga1 K3 147.0(3) . 2_666 ? K2 Ga1 K3 73.19(7) 1_655 2_666 ? K1 Ga1 K3 132.62(7) 1_655 2_666 ? K1 Ga1 K3 67.75(7) . 2_666 ? O3 Ga1 K2 67.2(2) . 1_645 ? O4 Ga1 K2 138.3(3) . 1_645 ? O7 Ga1 K2 103.8(2) . 1_645 ? O9 Ga1 K2 40.5(2) . 1_645 ? K2 Ga1 K2 148.95(8) 1_655 1_645 ? K1 Ga1 K2 102.72(6) 1_655 1_645 ? K1 Ga1 K2 58.29(6) . 1_645 ? K3 Ga1 K2 123.81(7) 2_666 1_645 ? O4 K1 O8 93.5(2) 1_455 2_655 ? O4 K1 O2 56.9(2) 1_455 . ? O8 K1 O2 100.3(3) 2_655 . ? O4 K1 O8 95.7(2) 1_455 . ? O8 K1 O8 89.0(2) 2_655 . ? O2 K1 O8 151.3(2) . . ? O4 K1 OW1 89.4(3) 1_455 2_656 ? O8 K1 OW1 151.2(3) 2_655 2_656 ? O2 K1 OW1 58.1(3) . 2_656 ? O8 K1 OW1 119.2(3) . 2_656 ? O4 K1 O6 151.0(2) 1_455 1_655 ? O8 K1 O6 57.5(2) 2_655 1_655 ? O2 K1 O6 124.6(2) . 1_655 ? O8 K1 O6 83.4(2) . 1_655 ? OW1 K1 O6 116.4(3) 2_656 1_655 ? O4 K1 O7 110.9(2) 1_455 . ? O8 K1 O7 54.5(2) 2_655 . ? O2 K1 O7 70.1(2) . . ? O8 K1 O7 134.6(2) . . ? OW1 K1 O7 97.8(3) 2_656 . ? O6 K1 O7 55.5(2) 1_655 . ? O4 K1 O10 117.3(2) 1_455 2_645 ? O8 K1 O10 129.3(3) 2_655 2_645 ? O2 K1 O10 129.9(3) . 2_645 ? O8 K1 O10 51.2(2) . 2_645 ? OW1 K1 O10 72.9(3) 2_656 2_645 ? O6 K1 O10 84.5(2) 1_655 2_645 ? O7 K1 O10 130.4(2) . 2_645 ? O4 K1 Te2 119.83(19) 1_455 2_655 ? O8 K1 Te2 31.59(16) 2_655 2_655 ? O2 K1 Te2 99.42(18) . 2_655 ? O8 K1 Te2 102.45(17) . 2_655 ? OW1 K1 Te2 126.5(2) 2_656 2_655 ? O6 K1 Te2 34.25(16) 1_655 2_655 ? O7 K1 Te2 32.42(14) . 2_655 ? O10 K1 Te2 118.68(18) 2_645 2_655 ? O4 K1 Te1 28.39(16) 1_455 . ? O8 K1 Te1 99.61(18) 2_655 . ? O2 K1 Te1 28.64(15) . . ? O8 K1 Te1 123.25(17) . . ? OW1 K1 Te1 70.8(2) 2_656 . ? O6 K1 Te1 146.64(18) 1_655 . ? O7 K1 Te1 91.85(15) . . ? O10 K1 Te1 127.02(18) 2_645 . ? Te2 K1 Te1 113.78(7) 2_655 . ? O4 K1 K2 140.30(19) 1_455 1_645 ? O8 K1 K2 125.05(18) 2_655 1_645 ? O2 K1 K2 102.29(18) . 1_645 ? O8 K1 K2 94.04(18) . 1_645 ? OW1 K1 K2 52.7(2) 2_656 1_645 ? O6 K1 K2 68.37(16) 1_655 1_645 ? O7 K1 K2 88.18(16) . 1_645 ? O10 K1 K2 46.87(16) 2_645 1_645 ? Te2 K1 K2 95.22(7) 2_655 1_645 ? Te1 K1 K2 122.79(8) . 1_645 ? O4 K1 Ga1 25.82(16) 1_455 1_455 ? O8 K1 Ga1 104.16(17) 2_655 1_455 ? O2 K1 Ga1 78.75(16) . 1_455 ? O8 K1 Ga1 72.63(16) . 1_455 ? OW1 K1 Ga1 90.7(2) 2_656 1_455 ? O6 K1 Ga1 150.46(18) 1_655 1_455 ? O7 K1 Ga1 136.13(17) . 1_455 ? O10 K1 Ga1 93.23(16) 2_645 1_455 ? Te2 K1 Ga1 135.36(8) 2_655 1_455 ? Te1 K1 Ga1 50.79(4) . 1_455 ? K2 K1 Ga1 129.04(8) 1_645 1_455 ? O4 K2 O5 57.2(2) 1_455 . ? O4 K2 O10 102.4(2) 1_455 2 ? O5 K2 O10 124.0(3) . 2 ? O4 K2 O9 140.0(2) 1_455 1_465 ? O5 K2 O9 91.1(2) . 1_465 ? O10 K2 O9 116.4(2) 2 1_465 ? O4 K2 O10 137.5(2) 1_455 1_565 ? O5 K2 O10 141.8(2) . 1_565 ? O10 K2 O10 90.4(2) 2 1_565 ? O9 K2 O10 55.5(2) 1_465 1_565 ? O4 K2 O8 90.3(2) 1_455 2_655 ? O5 K2 O8 105.4(2) . 2_655 ? O10 K2 O8 127.9(3) 2 2_655 ? O9 K2 O8 74.1(2) 1_465 2_655 ? O10 K2 O8 51.8(2) 1_565 2_655 ? O4 K2 O6 68.4(2) 1_455 2 ? O5 K2 O6 124.9(2) . 2 ? O10 K2 O6 58.0(2) 2 2 ? O9 K2 O6 141.2(2) 1_465 2 ? O10 K2 O6 85.7(2) 1_565 2 ? O8 K2 O6 81.9(2) 2_655 2 ? O4 K2 OW1 86.5(3) 1_455 2_566 ? O5 K2 OW1 56.2(3) . 2_566 ? O10 K2 OW1 72.5(3) 2 2_566 ? O9 K2 OW1 95.5(2) 1_465 2_566 ? O10 K2 OW1 135.8(3) 1_565 2_566 ? O8 K2 OW1 159.4(3) 2_655 2_566 ? O6 K2 OW1 115.5(3) 2 2_566 ? O4 K2 Ga1 27.56(16) 1_455 1_455 ? O5 K2 Ga1 77.01(17) . 1_455 ? O10 K2 Ga1 75.11(17) 2 1_455 ? O9 K2 Ga1 167.14(18) 1_465 1_455 ? O10 K2 Ga1 133.37(17) 1_565 1_455 ? O8 K2 Ga1 103.96(18) 2_655 1_455 ? O6 K2 Ga1 48.88(16) 2 1_455 ? OW1 K2 Ga1 82.10(19) 2_566 1_455 ? O4 K2 Te2 78.57(17) 1_455 2 ? O5 K2 Te2 121.17(18) . 2 ? O10 K2 Te2 28.98(16) 2 2 ? O9 K2 Te2 141.38(18) 1_465 2 ? O10 K2 Te2 96.93(16) 1_565 2 ? O8 K2 Te2 112.04(18) 2_655 2 ? O6 K2 Te2 31.60(16) 2 2 ? OW1 K2 Te2 87.24(19) 2_566 2 ? Ga1 K2 Te2 51.36(4) 1_455 2 ? O4 K2 Te1 28.84(15) 1_455 . ? O5 K2 Te1 28.42(16) . . ? O10 K2 Te1 117.29(19) 2 . ? O9 K2 Te1 115.85(17) 1_465 . ? O10 K2 Te1 149.03(18) 1_565 . ? O8 K2 Te1 97.84(18) 2_655 . ? O6 K2 Te1 97.05(17) 2 . ? OW1 K2 Te1 70.3(2) 2_566 . ? Ga1 K2 Te1 51.44(4) 1_455 . ? Te2 K2 Te1 101.38(6) 2 . ? O4 K2 Te2 156.32(19) 1_455 1_565 ? O5 K2 Te2 120.03(18) . 1_565 ? O10 K2 Te2 97.51(18) 2 1_565 ? O9 K2 Te2 28.94(15) 1_465 1_565 ? O10 K2 Te2 28.80(15) 1_565 1_565 ? O8 K2 Te2 67.19(17) 2_655 1_565 ? O6 K2 Te2 113.13(17) 2 1_565 ? OW1 K2 Te2 111.9(2) 2_566 1_565 ? Ga1 K2 Te2 161.89(8) 1_455 1_565 ? Te2 K2 Te2 115.72(7) 2 1_565 ? Te1 K2 Te2 142.84(8) . 1_565 ? OW1 K3 O7 92.9(3) . 2_666 ? OW1 K3 O5 152.9(3) . 2_666 ? O7 K3 O5 114.2(3) 2_666 2_666 ? OW1 K3 O2 142.0(3) . 2_666 ? O7 K3 O2 71.0(2) 2_666 2_666 ? O5 K3 O2 56.4(2) 2_666 2_666 ? OW1 K3 OW1 90.3(3) . 2_666 ? O7 K3 OW1 124.2(3) 2_666 2_666 ? O5 K3 OW1 76.4(3) 2_666 2_666 ? O2 K3 OW1 73.0(2) 2_666 2_666 ? OW1 K3 O1 67.1(3) . 2_656 ? O7 K3 O1 159.1(2) 2_666 2_656 ? O5 K3 O1 85.8(2) 2_666 2_656 ? O2 K3 O1 128.4(2) 2_666 2_656 ? OW1 K3 O1 64.2(2) 2_666 2_656 ? OW1 K3 O1 65.7(3) . 1_565 ? O7 K3 O1 71.6(2) 2_666 1_565 ? O5 K3 O1 123.1(2) 2_666 1_565 ? O2 K3 O1 76.5(2) 2_666 1_565 ? OW1 K3 O1 59.5(2) 2_666 1_565 ? O1 K3 O1 103.18(19) 2_656 1_565 ? OW1 K3 Te1 160.0(3) . 2_666 ? O7 K3 Te1 94.54(19) 2_666 2_666 ? O5 K3 Te1 27.94(16) 2_666 2_666 ? O2 K3 Te1 28.66(15) 2_666 2_666 ? OW1 K3 Te1 70.19(19) 2_666 2_666 ? O1 K3 Te1 106.31(16) 2_656 2_666 ? O1 K3 Te1 99.19(16) 1_565 2_666 ? OW1 K3 K2 140.8(3) . 2_666 ? O7 K3 K2 86.85(19) 2_666 2_666 ? O5 K3 K2 45.42(17) 2_666 2_666 ? O2 K3 K2 74.26(16) 2_666 2_666 ? OW1 K3 K2 121.8(2) 2_666 2_666 ? O1 K3 K2 104.92(18) 2_656 2_666 ? O1 K3 K2 148.04(17) 1_565 2_666 ? Te1 K3 K2 58.34(6) 2_666 2_666 ? OW1 K3 Te2 90.1(2) . 1_566 ? O7 K3 Te2 26.05(16) 2_666 1_566 ? O5 K3 Te2 113.20(19) 2_666 1_566 ? O2 K3 Te2 88.74(17) 2_666 1_566 ? OW1 K3 Te2 150.2(2) 2_666 1_566 ? O1 K3 Te2 141.59(18) 2_656 1_566 ? O1 K3 Te2 93.89(15) 1_565 1_566 ? Te1 K3 Te2 104.51(8) 2_666 1_566 ? K2 K3 Te2 72.99(8) 2_666 1_566 ? OW1 K3 Ga1 84.1(2) . 2_666 ? O7 K3 Ga1 24.24(16) 2_666 2_666 ? O5 K3 Ga1 121.43(19) 2_666 2_666 ? O2 K3 Ga1 66.97(17) 2_666 2_666 ? OW1 K3 Ga1 101.6(2) 2_666 2_666 ? O1 K3 Ga1 146.82(18) 2_656 2_666 ? O1 K3 Ga1 47.47(14) 1_565 2_666 ? Te1 K3 Ga1 95.20(9) 2_666 2_666 ? K2 K3 Ga1 107.86(9) 2_666 2_666 ? Te2 K3 Ga1 48.84(5) 1_566 2_666 ? OW1 K3 K3 49.9(2) . 2_666 ? O7 K3 K3 117.5(2) 2_666 2_666 ? O5 K3 K3 113.4(2) 2_666 2_666 ? O2 K3 K3 106.7(2) 2_666 2_666 ? OW1 K3 K3 40.46(19) 2_666 2_666 ? O1 K3 K3 54.12(15) 2_656 2_666 ? O1 K3 K3 49.06(16) 1_565 2_666 ? Te1 K3 K3 110.53(15) 2_666 2_666 ? K2 K3 K3 154.94(15) 2_666 2_666 ? Te2 K3 K3 131.64(14) 1_566 2_666 ? Ga1 K3 K3 94.98(14) 2_666 2_666 ? Te1 O1 Te1 100.9(3) . 2_556 ? Te1 O1 K3 129.2(3) . 2_656 ? Te1 O1 K3 106.6(3) 2_556 2_656 ? Te1 O1 K3 114.2(3) . 1_545 ? Te1 O1 K3 131.1(3) 2_556 1_545 ? K3 O1 K3 76.82(19) 2_656 1_545 ? Te1 O2 K1 105.0(3) . . ? Te1 O2 K3 101.3(3) . 2_666 ? K1 O2 K3 96.1(2) . 2_666 ? Ga1 O3 Te1 122.1(4) . 2_656 ? Ga1 O4 Te1 121.8(4) . 1_655 ? Ga1 O4 K1 114.3(3) . 1_655 ? Te1 O4 K1 109.4(3) 1_655 1_655 ? Ga1 O4 K2 108.6(3) . 1_655 ? Te1 O4 K2 107.3(3) 1_655 1_655 ? K1 O4 K2 90.8(2) 1_655 1_655 ? Te1 O5 K2 106.6(3) . . ? Te1 O5 K3 106.4(3) . 2_666 ? K2 O5 K3 87.5(2) . 2_666 ? Te2 O6 Te2 101.6(3) . 2 ? Te2 O6 K1 135.2(4) . 1_455 ? Te2 O6 K1 91.1(3) 2 1_455 ? Te2 O6 K2 97.7(3) . 2 ? Te2 O6 K2 151.2(4) 2 2 ? K1 O6 K2 90.1(2) 1_455 2 ? Ga1 O7 Te2 121.1(4) . 2_655 ? Ga1 O7 K3 118.0(3) . 2_666 ? Te2 O7 K3 114.9(3) 2_655 2_666 ? Ga1 O7 K1 104.1(3) . . ? Te2 O7 K1 90.9(3) 2_655 . ? K3 O7 K1 99.2(3) 2_666 . ? Te2 O8 K1 96.6(3) . 2_655 ? Te2 O8 K1 115.7(4) . . ? K1 O8 K1 91.0(2) 2_655 . ? Te2 O8 K2 153.0(4) . 2_655 ? K1 O8 K2 85.0(2) 2_655 2_655 ? K1 O8 K2 91.1(2) . 2_655 ? Ga1 O9 Te2 119.1(4) . 1_655 ? Ga1 O9 K2 114.6(3) . 1_645 ? Te2 O9 K2 104.9(3) 1_655 1_645 ? Te2 O10 K2 104.7(3) . 2 ? Te2 O10 K2 103.4(3) . 1_545 ? K2 O10 K2 89.6(2) 2 1_545 ? Te2 O10 K1 165.9(4) . 2_645 ? K2 O10 K1 82.0(2) 2 2_645 ? K2 O10 K1 88.9(2) 1_545 2_645 ? K3 OW1 K1 98.1(3) . 2_656 ? K3 OW1 K2 105.9(3) . 2_566 ? K1 OW1 K2 79.3(3) 2_656 2_566 ? K3 OW1 K3 89.7(3) . 2_666 ? K1 OW1 K3 144.2(4) 2_656 2_666 ? K2 OW1 K3 132.0(3) 2_566 2_666 ?